激光烧蚀微波诱导等离子体发射光谱法测定聚合物中的Cd、Pb和Zn

M. Ślachciński, Michał Janeda, H. Matusiewicz
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摘要

摘要研究了激光烧蚀微波诱导等离子体光谱法(LA-MIP OES)分析塑料材料的潜力。无机物质,例如金属,可以作为添加剂、抗氧化剂、稳定剂、增塑剂、着色剂和催化残留物、污染物加入其中,并且可能以各种浓度存在。研究发现,作为聚氯乙烯(PVC)和聚乙烯(PE)成分的微量元素(Cd、Pb和Zn)含量升高。采用266 nm激光烧蚀作为MIP OES的采样方法。将该系统所得到的聚合物样品在高压-高温聚焦微波加热消解系统和标准样品气动雾化(PN)分解后得到的结果与MIP OES光谱仪进行了比较。提出了以纤维素颗粒为支撑的LA-MIP OES测定聚合物中元素定性分析的校准策略。这种分析性能的LA-MIP OES系统的特点是确定的检出限(lod)和精密度(rsd)的元素被测试。同时测定Cd、Pb、Zn的实验浓度检出限分别为2µg g−1、3µg g−1和5µg g−1,其信号值为空白标准偏差(LOD、3σ空白判据、峰高)的3倍。该方法对微量样品分析具有较好的精密度(RSD为3% ~ 5%)。
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Determination of Cd, Pb and Zn in Polymers by Laser Ablation Microwave Induced Plasma Optical Emission Spectrometry
Abstract The potential of laser ablation microwave induced plasma optical emission spectrometry (LA-MIP OES) for the analysis of plastic materials has been investigated. Inorganic species, e.g., metals may be added to them as additives, anti-oxidising agents, stabilisers, plasticisers, colorants and catalytic residues, contaminants and may be present in a wide range of concentrations. The study revealed elevated content of trace elements (Cd, Pb and Zn) which are components of poly(vinyl chloride) (PVC) and polyethylene (PE). Laser ablation using wavelengths of 266 nm as a sampling method for MIP OES was used. The result achieved using elaborated system were compared with those obtained after polymer samples decomposition in high pressure-temperature focused microwave heating digestion system and standard sample pneumatic nebulisation (PN) to MIP OES spectrometer. The calibration strategy using cellulose pellets as support for qualitative analysis for element determination in polymers by LA-MIP OES was proposed. This analytical performance of the LA-MIP OES system was characterised by a determination of the limits of detection (LODs) and precision (RSDs) for elements tested. The experimental concentration detection limits for simultaneous determination, calculated as the concentration giving a signal equal to three times of the standard deviation of the blank (LOD, 3σblank criterion, peak height) were 2 µg g−1, 3 µg g−1 and 5 µg g−1 for Cd, Pb and Zn, respectively. The method offers relatively good precision (RSD ranged from 3 % to 5 %) for micro sampling analysis.
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